CN101105480A - Cigarette main flume volatile organic compound ingredient determination method - Google Patents
Cigarette main flume volatile organic compound ingredient determination method Download PDFInfo
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Abstract
A detection method of volatility organic compound ingredient in cigarette mainstream smoke comprises the following steps: (1) the entrapment of the volatility organic compound in the cigarette mainstream smoke: a XAD-4 absorption tube and a cold solvent are in tandem and entrap the volatility organic compound in the cigarette mainstream smoke; (2) the analysis of smoke sample: absorption material in the absorption tube is transferred into a chromatogram bottle; an extraction liquid and an internal standard are added in the chromatogram bottle and leach the absorption volatility organic compound; the absorption volatility organic compound is directly put into GC-MS to be detected; after the solution in the absorption bottle is added with the internal standard, the solution is directly put into GC-MS to be analyzed and detected; the summation of the amount of leached volatility organic compound and the amount of volatility organic compound in the solution is the total amount of the volatility organic compound in the cigarette mainstream smoke. Compared with the prior method, the method in the invention has more easy operation, only need the XAD-4 absorption tube and a tandem device of a cold solvent bottle and can effectively absorb all the main volatility organic compounds in the cigarette mainstream smoke; furthermore, the method in the invention has the advantages of sound repeatability and sound sensitivity; the method in the invention is also suitable for analysis of samples in large quantities.
Description
Technical field
The invention belongs to the new method of the capture and the analysis of volatile organic compounds in a kind of cigarette mainstream flue gas.This method utilizes XAD adsorption tube and cold solvent to capture main volatile organic compound ingredient in the main flume jointly, adopts gas chromatography-mass spectrum (GC-MS) coupling method to realize the assay determination of this class material in the cigarette mainstream flue gas.
Technical background
Contain a large amount of volatile organic compounds (VOC) in the cigarette mainstream flue gas, this class material is gaseous state or liquid state at normal temperatures, and is generally poisonous, and penetrating odor is arranged, inflammable and explosive.In 44 kinds of cigarette smoke objectionable constituent in the Hoffmann list, listing, volatile organic component has 6 kinds, be respectively 1,3-butadiene, isoprene, styrene, benzene, toluene, vinyl cyanide, wherein benzene is human carcinogen's thing, 1,3-butadiene, isoprene, styrene and vinyl cyanide are the possible carcinogenic substances of human body.In the reason of these materials generations of research, when forming mechanism and reducing their content, it is crucial setting up a kind of analysis test method accurately.
The method of analyzing at present the VOC composition in the world can be divided into four classes: (1) direct injected method; (2) cold solvent collecting method; (3) sampler bag collecting method and (4) adsorbent (thermal desorption) method.Wherein, cold solvent collecting method reappearance is better, is adopted by numerous tobacco enterprises and NGO, but often needs in the experimentation a plurality of receiving flasks capture flue gas of contacting, complex operation.Other several class methods then exist sensitivity low, the problem that reappearance is bad.Therefore, be necessary to develop the method for volatile organic compounds in a kind of easy and simple to handle, arresting efficiency is high, favorable reproducibility, sensitivity for analysis are high capture and the analysis of cigarette main flume.
Summary of the invention
The present invention improves at the deficiency that exists in the existing analytical technology just, and the assay method of volatile organic compounds in custom-designed a kind of cigarette mainstream flue gas, mainly be that XAD-4 adsorption tube and cold solvent are combined, the common volatile organic compounds that captures in the cigarette mainstream flue gas, and use gas chromatograph-mass spectrometer (GCMS) to carry out assay determination, method of the present invention is simple and convenient, favorable reproducibility, to the arresting efficiency height of target compound, assay determination is highly sensitive.
The objective of the invention is to be achieved through the following technical solutions: the assay method of volatile organic compounds may further comprise the steps in the cigarette mainstream flue gas of the present invention:
(1) capture of volatile organic compounds in the cigarette mainstream flue gas: with XAD-4 adsorption tube and cold solvent series combination, the volatile organic compounds when capturing cigarette smoking jointly in the main flume; XAD-4 is a kind of macroporous absorbent resin, and this type of adsorbent has reasonable adsorption effect to the compound more than the C5.In cold solvent absorbed, the arresting efficiency of toluene was lower, and simple XAD-4 adsorption tube is to toluene arresting efficiency height, and to 1, it is relatively poor that 3-butadiene, isoprene capture effect, and adsorption tube and cold soln absorption bottle are contacted, and then can realize effective capture of volatile organic compounds.
(2) analysis of flue gas sample: the sorbing material in the adsorption tube is transferred in the chromatogram bottle, adds extract and interior mark, fully vibration extracts the volatile organic compounds of adsorbing, and directly advances gas chromatograph-mass spectrometer (GCMS) then and detects; Behind the mark, directly advance the gas chromatograph-mass spectrometer (GCMS) analyzing and testing in solution in the absorption bottle adds, sum of the two is the total amount of the volatile organic compounds in the cigarette mainstream flue gas;
Gas chromatography-mass spectrometry analysis condition: adopt DB-624 (60m * 0.32mm * 1.8 μ m) capillary chromatographic column to separate injector temperature: 220 ℃, sample size 1 μ L, split ratio 15: 1, column flow rate 1.5mL/min, heating schedule:
, mass spectrum condition: EI source, ionization voltage 70eV, scan mode: SIM.
In above-mentioned capture step, cigarette smoking adopts the rotating disc type smoking machine according to the suction of YC/T 29-1996 specified standard condition, 10 cigarette of each experiment suction; Cold solvent is chosen as methanol solution or aqueous isopropanol, and wherein the cooling of solution is by absorption bottle being placed the dry ice that contains isopropyl alcohol realize, temperature≤-80 ℃.Be designated as D6-benzene or D8-toluene in selected.
This method is compared with the method that original cold soln captures the main flume volatile organic compounds, operate easier, only need the series device of an XAD-4 adsorption tube and a cold solvent bottle, just can realize that the whole of volatile organic compounds main in the main flume effectively absorb, and mensuration good reproducibility, highly sensitive, be applicable to the analysis of batch samples.
Description of drawings:
Accompanying drawing is the capturing device of the cigarette mainstream flue gas volatile organic compounds of the present invention's use.
Among the figure: 1. adsorption tube, 2. absorption bottle
Embodiment
The present invention is further described by the following examples, but does not limit the present invention.
Cigarette after balance and the screening is aspirated according to YC/T 29-1996 specified standard condition with the rotating disc type smoking machine, 10 cigarette of each experiment suction, behind drip catcher, connect the series device of an XAD-4 adsorption tube 1 and 10ml methyl alcohol cold soln absorption bottle 2, the common mainstream smoke gas phase object that captures, wherein the cooling of solution is by absorption bottle being placed the dry ice that contains isopropyl alcohol realize, temperature≤-80 ℃.
After the smoking experiment, take out smoke gas collecting apparatus.Add the D6-benzene inner mark solution of 100 μ L4mg/l in cold solvent, vibration is even, and the GC-MS that takes a sample rapidly analyzes.For the XAD-adsorption tube, then adsorbent wherein is transferred in the conical flask, add 10ml methanol solution and 100 μ L inner mark solutions, after the vibration evenly, get upper strata liquid and advance the GC-MS analysis.The two measures the total amount that summation is the volatile organic compounds in the cigarette mainstream flue gas.Adopt this technology that certain trade mark cigarette is measured, the result is as shown in the table:
| |
1,3-butadiene | Isoprene | Vinyl cyanide | Benzene | Toluene |
| Measurement result (ug/ props up) | 30.2 | 292.4 | 6.6 | 36.5 | 63.0 |
Described step (capture method 1) according to embodiment 1 is measured certain trade mark cigarette, and with first absorption bottle after adsorption tube (capture method 2), two adsorption tubes polyphones (capture method 3) and two solvent bottles polyphone (capture method 4) these several flue gas trapping method measurement results compare, the result is as shown in the table:
| Capture method | Measurement result (ug/ props up) | ||||
| 1,3-butadiene | Isoprene | Vinyl cyanide | Benzene | Toluene | |
| 1 | 34.6 | 240.4 | 8.5 | 47.8 | 77.6 |
| 2 | 33.9 | 213.5 | 8.6 | 45.9 | 55.3 |
| 3 | 2.4 | 78.5 | 3.0 | 38.3 | 69.7 |
| 4 | 34.1 | 242.4 | 8.0 | 39.2 | 50.1 |
By data in the table as can be seen, than other several capture methods, this technology can capture volatile organic compounds important in the flue gas preferably.In addition, this technique reproducible is fine, operates also very simply, is applicable to the analysis of batch samples.
Claims (4)
1. the assay method of volatile organic compound ingredient in the cigarette mainstream flue gas is characterized in that: may further comprise the steps:
(1) capture of volatile organic compounds in the cigarette mainstream flue gas: with XAD-4 adsorption tube and cold solvent series combination, the volatile organic compounds when capturing cigarette smoking jointly in the main flume;
(2) analysis of flue gas sample: the sorbing material in the adsorption tube is transferred in the chromatogram bottle, adds extract and interior mark, fully vibration extracts the volatile organic compounds of adsorbing, and directly advances gas chromatograph-mass spectrometer (GCMS) then and detects; Behind the mark, directly advance the gas chromatograph-mass spectrometer (GCMS) analyzing and testing in solution in the absorption bottle adds, sum of the two is the total amount of the volatile organic compounds in the cigarette mainstream flue gas;
Gas chromatography-mass spectrometry analysis condition: adopt DB-624 (60m * 0.32mm * 1.8 μ m) capillary chromatographic column to separate injector temperature: 220 ℃, sample size 1 μ L, split ratio 15: 1, column flow rate 1.5mL/min, heating schedule:
Mass spectrum condition: EI source, ionization voltage 70eV, scan mode: SIM.
2. the assay method of volatile organic compound ingredient in the cigarette mainstream flue gas according to claim 1, it is characterized in that: in capturing step, cigarette smoking adopts the rotating disc type smoking machine according to the suction of YC/T29-1996 specified standard condition, 10 cigarette of each experiment suction.
3. the assay method of volatile organic compound ingredient in the cigarette mainstream flue gas according to claim 1, it is characterized in that: cold solvent is chosen as methanol solution or aqueous isopropanol, wherein the cooling of solution is by absorption bottle being placed the dry ice that contains isopropyl alcohol realize, temperature≤-80 ℃.
4. the assay method of volatile organic compound ingredient in the cigarette mainstream flue gas according to claim 1 is characterized in that: interior mark is selected D6-benzene or D8-toluene.
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